HCID 18961145, compound → HCID 3028825, compound

HRID 1708168Notes

Reaction equation

HRID 1708168 reaction equation
Cl[C:2]1[N:6]([CH3:7])[CH:5]=[N:4][C:3]=1[S:8]([NH:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][NH:18][S:19]([C:22]1[N:23]=[CH:24][N:25]([CH3:28])[C:26]=1Cl)(=[O:21])=[O:20])(=[O:10])=[O:9]>[OH-].[Na+].[Pd]>[CH3:28][N:25]1[CH:26]=[C:22]([S:19]([NH:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][NH:11][S:8]([C:3]2[N:4]=[CH:5][N:6]([CH3:7])[CH:2]=2)(=[O:9])=[O:10])(=[O:20])=[O:21])[N:23]=[CH:24]1

Participants

4

Reactant 1

HCID 18961145HCID 18961145, compound

Product 1

HCID 3028825HCID 3028825, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 14798Sodium HydroxideSolvent

Procedure

13 g (27 mmol) of 1,6-bis(5-chloro-1-methyl-4-imidazolesulfonamido)hexane from Example 47 in 250 ml of 1N sodium hydroxide solution are hydrogenated over 3 g of 10% strength Pd/C catalyst while shaking at an initial pressure of 3.45 bar until absorption of hydrogen is complete. After separating off the catalyst, the filtrate is evaporated in vacuo. The residue was recrystallized from water/methanol in order to give the title compound as colorless crystals of melting point 153°-154° C.

Workup

  1. customuntil absorption of hydrogen
  2. customAfter separating off the catalyst
  3. customthe filtrate is evaporated in vacuo
  4. customThe residue was recrystallized from water/methanol in order

Sources & evidence

ORD record
ord-7c442f48c0964b118a0f24fdf69fcdea
Source dataset
uspto-grants-1994_10
Patent number
US05356922

Reaction notes

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